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0 °C

A solution of 2-bromoanisole (50 g, 0,267 mol) in ether is added portionwise to a mixture of magnesium (7.1 g, 0,293 mol) in ether. After the addition is complete, the reaction mixture is heated at reflux for 1 hour, diluted with ether, cooled to 0° C., treated with a solution of 2-chloro-5-nitrobenzaldehyde (39 g, 0.210 mol) in tetrahydrofuran, warmed to room temperature and diluted with an ice/water mixture. After acidifying the aqueous mixture with hydrochloric acid (pH2-pH3), the organic phase is separated and the aqueous phase is extracted with ether. The extracts are combined, washed sequentially with 10% sodium hydrogen carbonate solution and brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the title product as a brown gum.

1. additionAfter the addition
2. temperaturethe reaction mixture is heated
3. temperatureat reflux for 1 hour
4. temperaturewarmed to room temperature
5. customthe organic phase is separated
6. extractionthe aqueous phase is extracted with ether
7. washwashed sequentially with 10% sodium hydrogen carbonate solution and brine
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated in vacuo